Plasma Surface Engineering

Santiago Corujeira Gallo

Universidade de Caxias do Sul

September 2009
 Birmingham - UK

Founded in middle age (7th century)

Population ca 2,500,000
Traditional industrial centre
Cultural diversity

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University of Birmingham
Founded in 1900

Research oriented
Ranked 12th in UK (RAE)

Multicultural
over 4000 Intl students
from 150 countries

Colleges
Arts and Law
Engineering and Physical Sciences
Life and Environmental Sciences
Medical and Dental Sciences
Social Sciences
Surface Engineering Group (2007)
Composition of the group:
1 Professor
1 Senior Lecturer / Reader
2 Research fellows
1 Visiting research fellow
7 PhD students
2 MSc students
2 Undergraduate students

Topics of research:
- Plasma diffusion treatments
- Thermal oxidation
- PVD coatings
- Nanoindentation
Active screen plasma surface engineering
of austenitic stainless steel for enhanced
tribological and corrosion properties

• Austenitic stainless steel

• Plasma surface engineering

• Tribological and corrosion properties

• Active screen
 Austenitic stainless steel
• Typical composition: 18% Cr – 8% Ni
• AISI 316: 17% Cr – 12% Ni – 2% Mo

Typical properties:
• Excellent corrosion resistance
• Non-magnetic
• No ductile-to-brittle transition
• Poor mechanical properties
• Low wear resistance
Surface engineering treatments

Benefits of surface engineering

• Improved performance
• Use cheaper materials
• Increase design flexibility

Diffusion treatments:
• No sharp interface - gradient
• Slow (temperature – time)
 Plasma surface engineering
C or N containing gas

Conventional gas nitriding ~ 550oC

Treated substrate
Conventional gas carburising ~ 950oC

C or N containing gas
at low pressure

- -
Cr23C6
+

Cr1-2N -
Treated substrate - cathode (-)
GDOES composition depth profiles
XRD - phase identification

S-phase
or
expanded
austenite
 Micrographs of expanded austenite

Typical cross section

optical micrograph

Typical top view

SEM micrograph
 Microhardness testing
Typical instrumented
hardness test curves

Typical load
bearing capacity
 Microhardness indents
Tough carbon
expanded austenite

Brittle nitrogen
expanded austenite
 Wear testing

Dry sliding pin-on-disc test, 10 N normal load, WC

counterpart, 0.03 m/s sliding speed; 4.5 hours
 Wear results
AISI 316 UT AISI 316 PC
Morphology of the wear tracks

AISI 316 UT AISI 316 PC

Wear track of AISI 316 UT
Wear track of AISI 316 PC
 Wear debris

Untreated sample: metallic debris Treated sample: oxide debris

Wear debris Colour Size Magnetic Possible phases

Treated Red / Orange <20um No alpha-Fe2O3 Hematite
Un treated Black >20um Yes Fe3O4 Magnetite
Wear debris – TEM SAD pattern
 Wear conclusions

• The wear resistance of carbon expanded austenite

is 2 orders of magnitude higher than AISI 316 UT

• The wear mechanism changes from adhesive wear

in AISI 316 UT to oxidational wear in AISI 316 PC

• The layer of carbon expanded austenite reduces

the subsurface deformation and supports the
protective oxide layer
Corrosion testing

Immersion corrosion
Boiling H2SO4 (16%)
1 to 20 hours
 Corrosion results
AISI 316 UT AISI 316 PC

After 1 hour immersed in boiling sulphuric acid (16%)

Corrosion mechanisms
Corrosion mechanisms - Schematic
 Macrographs of corroded samples
AISI 316 UT AISI 316 DCPC AISI 316 ASPC

AISI 316 DCPC AISI 316 ASPC

Macrographs
“as treated”
 Corrosion conclusions

• Carbon expanded austenite exhibits higher corrosion

resistance to boiling sulphuric acid than AISI 316 UT

• The corrosion mechanisms are defect-controlled

(MnS inclusions, slip bands and grain boundaries)

• The AS treated samples performed better than the

DC ones through the elimination of edge effects
 Active screen plasma treatments

Active Screen experimental

setting inside a conventional
DC plasma furnace / reactor

Nitriding mechanisms of
Active Screen - schematics
DC and AS plasma reactors
Industrial AS plasma furnace
AS typical treatment cycle
Processing conditions
 Benefits of AS treatment
DC – edge effect DC – arcing damage AS – feature less

AS –rusty components before ASPN AS – rusty components after ASPN

 Active Screen conclusions

• AS plasma treatments can produce superior

surface quality than DC treatments (no edge effect or
arcing damage)

• AS treatments are less sensitive to the surface

condition of components (rust, oil, etc.)

• AS plasma shows potential to further improve the

results obtained with DC or other plasma treatments
 Acknowledgements

This project was sponsored by:

EU scholarships for Latin America

Techint group
The University of Birmingham

Universidad Tecnológica Nacional

Thank you very much indeed